SN/QC/SAPP/024

Department Quality Control Issue # 0 3

Section Quality Control Issue Date 1 1 - 2 0 1 9
THIS DOCUMENT IS NOT VALID WITHOUT SIGNATURES
STANDARD ANALYTICAL PROCEDURE HARICAM 7.5 MG TABLET

PROCEDURE FOR ANALYSIS OF

HARICAM 7.5MG TABLETS
(MELOXICAM 7.5MG TABLET)
(USP SPECS)

DRN …… 056389

AMENDMENT SHEET

INITIATED
REV. # DATE PAGE # NATURE OF AMENDMENT DONE BY
BY
00 05.06.2007 USMAN ALL New Introduction
01 23.05.2013 SIRAJ ALL Updated as per Pharmacopeia
Formatting , Header and Footer,
02 03.03.2015 SIRAJ ALL
Page numbering
Formatting, Header and Footer,
03 04.11.2019 HURRYAM ALL
Addition of Technical section

WRITTEN BY QC OFFICER

REVIEWED BY SENIOR QC OFFICER

APPROVED BY QC MANAGER

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SN/QC/SAPP/024
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 1 1 - 2 0 1 9
THIS DOCUMENT IS NOT VALID WITHOUT SIGNATURES
STANDARD ANALYTICAL PROCEDURE HARICAM 7.5 MG TABLET

CONTENTS

1.0 AMENDMENT ……………………………………………..…01

2.0 PURPOSE…………………………………………………..…03

3.0 SCOPE…………………………………………………….…...03

4.0 PROCEDURE ……………………………………………...…03

5.0 RESPONSIBILITY …………………………………………...03

6.0 PRODUCT SPECIFICATIONS ………………………….....03

7.0 TESTS …………………………………………………….…...03

7.1 INSTRUMENTS..………………………………….….03

7.2 REAGENTS .……………………………………….…03

8.0 COMPOSITION…………………………………………….....04

9.0 IDENTIFICATION…………………………………………......04

10.0 CHEMICAL ANALYSIS…………………………………........04

10.1 DISSOLUTION……………………………………..…04

10.2 ASSAY……………………………….………………...04

10.2.1 BY UV …………………………………………....…..04

10.2.3 BY HPLC………………………………………....…...06

10.2.4 CONTENT UNIFORMITY ……………………….…...07

11.0 DOCUMENTATION ...………………………………...……...07

12.0 REFERENCE ……...............................................................08

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 SN/QC/SAPP/024
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 1 1 - 2 0 1 9
THIS DOCUMENT IS NOT VALID WITHOUT SIGNATURES
STANDARD ANALYTICAL PROCEDURE HARICAM 7.5 MG TABLET

2.0 PURPOSE
This document is established to define the method of analysis for incoming product Haricam 7.5mg tablets to
confirm its physical and chemical properties.

3.0 SCOPE
This procedure is applicable in the Quality Control Department for the analysis of Incoming Haricam 7.5 mg
tablets.

4.0 PROCEDURE
Collect the sample according to sampling procedure (sop number SN/QC/SOP/021) and analyze it according
to the standard analytical procedure.

5.0 RESPONSIBILITY:

ANALYST

MANAGER Q.C

6.0 PRODUCT SPECIFICATIONS

Sr. # PARTICULARS AFTER MIXING AFTER AFTER COATING/

COMPRESSION FINISHED
1. Physical Off white to white White color A white color Film
Appearance granules. Core tablet. coated tablet.
2. Identification Must be positive Must be positive Must be positive

3. Average weight 180mg ± 2% - -

3. Loss on drying NMT 5 % - -

4. Disintegration - NMT 15 min NMT 30min.

Time
5. Friability - NMT 1.0% -
6. Hardness - NLT 4.0 Kg -
7. Diameter - 8.0mm + 0.5mm 8.5mm + 0.5mm
8 Dissolution - NLT 80% NLT 80%
9 Thickness - 3.0 + 0.5 mm 3.5 + 0.5 mm
10 Assay Limit 90 – 110%

7.0 TESTS

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Department Quality Control Issue # 0 3
Section Quality Control Issue Date 1 1 - 2 0 1 9
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STANDARD ANALYTICAL PROCEDURE HARICAM 7.5 MG TABLET
7.1 Instruments
a) Volumetric Flask 50 ml, 100ml
b) Beakers
c) Test Tubes
d) Pipette 1, 2 ,10ml
e) Electric Balance
f) Melting Point Apparatus
g) Spectrophotometer
7.2 Reagents/Chemicals
a) Distilled Water
b) Methanol
c) 0.1N NaOH.
d) Potassium dihydrogen phosphate
e) 0.5 M sodium hydroxide
f) 1M sodium hydroxide 
g) 2-amino-5-methylthiazole 
h) Diammonium hydrogen  orthophosphate
i) Orthophosphoric acid

8.0 COMPOSITION:

Each film coated tablet contains:

Meloxicam BP…………………7.5mg.
(Product Specs: BP)

9.0 IDENTIFICATION:

The retention time of the major peak in the chromatogram of the Assay preparation corresponds to that in the
chromatogram of the Standard preparation, as obtained in the Assay.

10.0 Chemical Analysis

10.1 Dissolution: 
Apparatus 2: 75rpm
Time: 30minutes
Medium: pH 7.5 phosphate buffer (prepared by dissolving 6.81g of potassium dihydrogen phosphate in
800ml of water, adjust the pH to 7.5 with 0.5 M sodium hydroxide, and diluting with water to 1 liter); 900ml.

Standard solution:
TEXT TECHNICAL
Weigh accurately Meloxicam equivalent to 0.1g (eqv. To 100mg) 100ml
100 mg Meloxicam RS and dissolve in 100
mL of phosphate buffer. Stir for about 5 to 10 0.8ml 100ml
min. Then take 0.8 mL from the above
solution and dissolve in 100 mL with the same ʎ = 362 nm
solvent. Sonicate for about 5 to 10 min then
scan the solution at 362 nm.

Sample solution:

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SN/QC/SAPP/024
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 1 1 - 2 0 1 9
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STANDARD ANALYTICAL PROCEDURE HARICAM 7.5 MG TABLET
Add one tablet in each basket, volume of ʎ= 362 nm
900mL phosphate buffer and take 100mL of
Tolerances: Not less than 80% of the labeled amount of Meloxicam is dissolved in 30minutes.

10.2 ASSAY:
10.2.1 After final mixing (By UV):
Sample solution:
TEXT TECHNICAL
Take granules and weigh them. Crush the 0.48g (eqv. To 20mg) 100 ml
granules and weigh accurately 180 mg
equivalent to 20 mg sample and dissolve in 10ml 100 ml
100 mL of 0.1N NaOH. Stirr for about 5 to 10
min. Take 10 mL from the above solution and ʎ = 362nm
dissolve in 100 mL with the same solvent.
Sonicate for about 5 to 10 min. Scan the
solution at 362 nm.

Standard solution:
TEXT TECHNICAL
Weigh accurately Meloxicam equivalent to 20 0.02g (eqv. To 20mg) 100ml
mg Meloxicam RS and dissolve in 100 mL of
0.1 N NaOH. Stir for about 5 to 10 min. Then 10ml 100ml
take 10 mL from the above solution and
dissolve in 100 mL with the same solvent. ʎ = 362 nm
Sonicate for about 5 to 10 min then scan the
solution at 362 nm.

OBSERVATION AND CALCULATIONS

%age = ABSORBANCE OF SAMPLE X 100

ABSORBANCE OF STANDARD

LIMIT: 90 ---------- 110 %

10.2.2 Assay for tablets (By UV):
Sample solution:
TEXT TECHNICAL
Take 20 tablets and weigh them. Crush the 0.48g (eqv. To 20mg) 100 ml
tablets and weigh accurately 180 mg
equivalent to 20 mg sample and dissolve in 10ml 100 ml
100 mL of 0.1N NaOH. Stirr for about 5 to 10
min. Take 10 mL from the above solution and ʎ = 362nm
dissolve in 100 mL with the same solvent.
Sonicate for about 5 to 10 min. Scan the
solution at 362 nm.

Standard solution:
TEXT TECHNICAL
Weigh accurately Meloxicam equivalent to 20 0.02g (eqv. To 20mg) 100ml
mg Meloxicam RS and dissolve in 0 mL of 0.1
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SN/QC/SAPP/024
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 1 1 - 2 0 1 9
THIS DOCUMENT IS NOT VALID WITHOUT SIGNATURES
STANDARD ANALYTICAL PROCEDURE HARICAM 7.5 MG TABLET
N NaOH. Stir for about 5 to 10 min. Then take 10ml 100ml
10 mL from the above solution and dissolve in
100 mL with the same solvent. Sonicate for ʎ = 362 nm
about 5 to 10 min then scan the solution at
362 nm.

OBSERVATION AND CALCULATIONS

%age = ABSORBANCE OF SAMPLE X 100

ABSORBANCE OF STANDARD

LIMIT: 90 ---------- 110 %

10.2.3 (By HPLC)

Chromatographic system:
Mode: LC
Detector: UV 254nm
Column: 4-mm×10-cm; packing L1
Flow rate: 1mL/min
Injection: 25uL
Solution A: Dissolve 2g of dibasic ammonium phosphate in 1L of water, and adjust with phosphoric acid to
a Ph of 7.0 ± 0.1.
Solution B: Mix 650mL of methanol and 100mL of isopropyl alcohol.
Mobile phase: Prepare a filtered and degassed mixture of Solution A and Solution B(63:37).

Standard stock preparation:

TEXT TECHNICAL
Transfer 50mg of USP Meloxicam RS, 0.05g (eqv. To 50mg) (1mL 1N
accurately weighed, to a 50mL volumetric NaOH+30ml methanol)50Ml(methanol)
flask, dissolved in 1mL of 1N sodium
hydroxide and 30mL of methanol, and dilute
10ml 100ml(methanol)
with methanol to volume. Transfer 10mL of the
resulting solution to a 100mL volumetric flask,
add 10mL of 1N sodium hydroxide, and dilute
with methanol to volume.

Standard solution:
TEXT TECHNICAL
Transfer 15mL of the standard stock solution 15mL (standard stock solution)
to a 25mL volumetric flask, and dilute with 25mL water.
water to a volume.

Assay stock solution:

TEXT TECHNICAL
Transfer 10 tablets to a 1000mL volumetric
flask, add about 100 mL of 1N NaOH , shake
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 SN/QC/SAPP/024
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 1 1 - 2 0 1 9
THIS DOCUMENT IS NOT VALID WITHOUT SIGNATURES
STANDARD ANALYTICAL PROCEDURE HARICAM 7.5 MG TABLET
to disperse the tablets, and add 800mL of 10 tablets 1000mL (100 mL
methanol. Sonicate the solution for about 15 NaOH+800 mL methanol)
minutes, then stirr for 30 minutes. Dilute with
methanol to volume, and mix. Filter the
solution and use filtrate.

Assay preparation:
TEXT TECHNICAL
Transfer 15 mL of the Assaay stock solution to
a 25 mL volumetric flask, and dilute with water 15mL (assay stock solution)
to volume. 25mL water.

Calculate the quantity, in mg, of Meloxicam(C14H13N3O4S2)  in the proportion of Tablets taken by the formula:
5000(C/3) (ru/rs)
C= the concentration, in mg per mL, of USP Meloxicam RS in the Standard preparations.
Ru= peak responses obtained from the Assay preparation
Rs= peak responses obtained from the Standard preparation

10.3 Content uniformity:

Sample:
TEXT TECHNICAL
Accurately weigh 10 tablets individually. 1 tablet(7.5mg) 100ml
Calculate the drug Substance content,
expressed as % of label claim, of each tablet
from the weight of the individual tablet and 14ml 100ml
the result of the Assay. Calculate the
acceptance value. Add one tablet in each
flask and add 0.1N NaOH to dissolve the
tablet and Sonicate it until whole of the tablet ʎ = 362nm
get dissolve and make up volume upto 100ml.
Then take 14 mL from the above solution and
dissolve in 100 mL with the same solvent.
Filter the solution and calculate the
absorbance at 362nm.

Standard solution:
TEXT TECHNICAL
Dissolve 50mg of Meloxicam working standard 50mg 50 ml
in 0.1N NaOH and dilute to 50ml with the
same reagent. Sonicate the solution for 10
minutes. Filter, if necessary, and dilute 1 ml of 1ml 50 ml
the filtrate to 50 ml with methanol. Scan the
ʎ = 362nm
solution at 262nm.

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SN/QC/SAPP/024
Department Quality Control Issue # 0 3
Section Quality Control Issue Date 1 1 - 2 0 1 9
THIS DOCUMENT IS NOT VALID WITHOUT SIGNATURES
STANDARD ANALYTICAL PROCEDURE HARICAM 7.5 MG TABLET

11.0 DOCUMENTATION
 Request for Analysis
 Certificate of Analysis
 Inprocess Register
 Instrument Log Books

12.0 REFERENCE:

USP 40: Volume 4. Page 4995